Hydrochloric Acid → HCID 11460950, Verbindung

HRID 488980

Reaktionsgleichung

Reaktionsgleichung von HRID 488980
CC(CC)[O-].CC(CC)[O-].CC(CC)[O-].[Al+3].C1(O)CCCCC1.[CH3:24][C:25]1[CH:26]=[CH:27][C:28]2[CH:29]=[C:30]3[C:43]([C:44](=O)[C:45]=2[CH:46]=1)=[CH:42][C:41]1[C:32]([C:33](=O)[C:34]2[C:39]([CH:40]=1)=[CH:38][CH:37]=[C:36]([CH3:48])[CH:35]=2)=[CH:31]3.Cl>C1COCC1.CC(C)=O>[CH3:24][C:25]1[CH:26]=[CH:27][C:28]2[C:45](=[CH:44][C:43]3[C:30]([CH:29]=2)=[CH:31][C:32]2[C:41](=[CH:40][C:39]4[C:34]([CH:33]=2)=[CH:35][C:36]([CH3:48])=[CH:37][CH:38]=4)[CH:42]=3)[CH:46]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric Acid2×HCID 7966CyclohexanolHCID 61289Aluminum sec-butoxideHCID 22269443HCID 22269443, Verbindung

Produkt 1

HCID 11460950HCID 11460950, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
145 °C

Versuchsvorschrift

To a 500 mL three necked round bottom flask with a thermometer, and a distillation head was added 32.76 grams of aluminum tri(sec-butoxide) and 200 mLs of cyclohexanol. To this was added 9 grams 3,10-Dimethylpentacene-5,12-dione. The reaction mixture was heated to 145° C. At 140° C., 8.7 grams of a distillate was collected. The reaction mixture was heated at 140° C. for 43 hours and cooled to room temperature. A solid was isolated by centrifugation. The supernate liquid was poured off and the solid was slurried with 140 mLs of 1N HCl and isolated on a Buchner funnel. The solid was slurried three times with 100 mLs each 1N HCl and the solvent was poured off each time. The solid was slurried three times with 100 mLs of acetone and isolated by filtration. The solid was slurried three times with 100 mLs of THF and isolated by filtration. The residue was air dried to give 2,9-dimethylpentacene.

Aufarbeitung

  1. distillationAt 140° C., 8.7 grams of a distillate was collected
  2. temperatureThe reaction mixture was heated at 140° C. for 43 hours
  3. temperaturecooled to room temperature
  4. customA solid was isolated by centrifugation
  5. additionThe supernate liquid was poured off
  6. customisolated on a Buchner funnel
  7. additionthe solvent was poured off each time
  8. customisolated by filtration
  9. customisolated by filtration
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f284e0ee4ae84db88b9349c17cf1dbc0
Quelldatensatz
uspto-grants-2005_12
Patentnummer
US06974877B2

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